CN102167884A - Preparation method of three-dimensional woven carbon fiber reinforced polyetheretherketone composite material - Google Patents
Preparation method of three-dimensional woven carbon fiber reinforced polyetheretherketone composite material Download PDFInfo
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- CN102167884A CN102167884A CN 201110020980 CN201110020980A CN102167884A CN 102167884 A CN102167884 A CN 102167884A CN 201110020980 CN201110020980 CN 201110020980 CN 201110020980 A CN201110020980 A CN 201110020980A CN 102167884 A CN102167884 A CN 102167884A
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Abstract
The invention relates to a preparation method of a three-dimensional woven carbon fiber reinforced polyetheretherketone composite material and belongs to a three-dimensional woven carbon fiber composite material technology. The preparation method comprises the following steps of: mixing polyetheretherketone fiber and carbon fiber according to a carbon fiber volume ratio; performing three-dimensional five-direction mixed weaving to prepare a prefabricated member; performing oxidation treatment on the prefabricated member sequentially; paving the prefabricated member in a mould; heating and pressurizing the mould; preserving the heat; heating the mould to 380 to 420 DEG C; pressurizing the mould and then preserving the heat; and cooling and demoulding to obtain the three-dimensional woven carbon fiber reinforced polyetheretherketone composite material. The preparation method has the advantages of combination of a three-dimensional weaving technology and a hot pressing method and simple process. The prepared three-dimensional woven carbon fiber reinforced polyetheretherketone composite material has excellent properties such as creep resistance, heat and humidity resistance, ageing resistance, wear resistance and the like.
Description
Technical field
The present invention relates to is a kind of preparation method of 3 D weaving carbon fiber reinforced polyether ether ketone matrix material, belongs to the 3 D weaving carbon fiber composite technology.
Background technology
D braided composites is a kind of advanced composite material that recent two decades is born, the intensity that can globality improves material significantly, fundamentally overcome low, the easy stratified shortcoming of tradition stratum plywood interlaminar shear strength, be widely used in fields such as aerospace, medical treatment and physical culture.Carbon fiber is by the carbon content height, and the artificial man-made fiber of fused not in heat treatment process is made through technologies such as thermally-stabilised oxide treatment, carbonizing treatment and greyings.Its profile has significant anisotropism, shows very high intensity along fiber direction, and carbon fiber proportion is little, therefore has very high specific tenacity.Simultaneously carbon fiber also has excellent specific properties such as high temperature resistant, rub resistance, corrosion-resistant and anti-irradiation.So carbon fiber has broad application prospects as the matrix material that strengthens body, both can be used as the structured material bearing load, can be used as functional materials again and plays a role.Polyether-ether-ketone (PEEK) resin is a kind of high performance thermoplastic resin, has high temperature resistant, corrosion-resistant, rub resistance, anti-irradiation and extremely outstanding mechanical property.In addition, PEEK easily extrudes and injection molding, good processability, and shaping efficiency is higher, so PEEK has application extremely widely in fields such as aerospace, automobile, boats and ships, oil and medical treatment.Yet traditional 3 D weaving carbon fiber reinforced composite is to adopt resin transfer moulding (RTM) prepared, the used resin matrix overwhelming majority is a thermosetting resin, because PEEK is a thermoplastic resin, there is big difficulty so adopt RTM to prepare 3 D weaving carbon fiber reinforced polyether ether ketone matrix material.3 D weaving carbon fiber reinforced polyether ether ketone matrix material will obtain important application in fields such as aerospace, automobile, oil, machinery and boats and ships if can prepare successfully.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of 3 D weaving carbon fiber reinforced polyether ether ketone matrix material.This method is prepared the sufficient 3 D weaving carbon fiber reinforced polyether ether ketone of fiber impregnation matrix material, and prepared 3 D weaving carbon fiber reinforced polyether ether ketone matrix material has good mechanical performance and wide application prospect.
The present invention is realized that by the following technical programs a kind of preparation method of 3 D weaving carbon fiber reinforced polyether ether ketone matrix material is characterized in that may further comprise the steps:
1) polyetheretherketonefiber fiber and carbon fiber are accounted for cumulative volume according to carbon fiber and make prefabricated component to shuffling, braid angle θ=25 ° than for 15-60% carries out three-dimensional five.To weave good prefabricated component then is (the NH of 3-10wt% in concentration
4)
2HPO
4Carry out oxide treatment in the solution, take out after boiling 0.5-1.5h, with deionized water rinsing and dry.
2) the three-dimensional shuffling oxidation prefabricated component that step 1) is made is laid in the mould, then mould is put into the heating under vacuum jar, and being 120-170 ℃ in temperature is 10-100kPa with vacuum pressure, and insulation 1-3h obtains the three-dimensional shuffling oxidation of exsiccant prefabricated component.
3) to step 2) to rise to temperature with the temperature rise rate of 10-20 ℃/min be 380-420 ℃ for the exsiccant prefabricated component that obtains, insulation 30-50min, the 0.3-0.8MPa that pressurizes then continues insulation 30-50min.
When 4) sample that step 3) is obtained was cooled to 150-180 ℃ with the rate of temperature fall of 0.5-2 ℃/min, the demoulding obtained 3 D weaving carbon fiber reinforced polyether ether ketone matrix material when continuing cooling again and being lower than 100 ℃.
The invention has the advantages that adopt the 3 D weaving technology to combine with hot-press method, process is simple, has successfully prepared in apparent good order and condition and the sufficient 3 D weaving carbon fiber reinforced polyether ether ketone of fiber impregnation matrix material.This matrix material as body material, as strengthening body, when having favorable comprehensive mechanical property, has performances such as excellent creep resistance, moisture-proof heat, ageing-resistant, antifriction damage with high-strength carbon fiber with the thermoplastic resin PEEK of excellent performance.
Description of drawings
The carbon fiber volume content that Fig. 1 prepares for example 1 of the present invention is 18% 3 D weaving carbon fiber reinforced polyether ether ketone matrix material microscopic appearance figure.
The carbon fiber volume content that Fig. 2 prepares for example 2 of the present invention is 36% 3 D weaving carbon fiber reinforced polyether ether ketone matrix material microscopic appearance figure.
Embodiment
Example 1
With carbon fiber volume amount be 18% and PEEK fiber volume amount be 82% blend fiber, ° carry out three-dimensional five by braid angle θ=25 and make the prefabricated component of long 1m, wide 12mm to braiding.Then prefabricated component is put into the (NH that concentration is 3wt%
4)
2HPO
4After boiling 1.5h in the solution, wash repeatedly, be 80 ℃ at oven temperature and carry out drying with deionized water.To cut and be laid in the pre-prepd mould through the three-dimensional shuffling fiber preform of oxide treatment, mould is put into the heating under vacuum jar, and Heating temperature is 170 ℃, and beginning to continue to be evacuated down to vacuum tightness is 80kPa, and under this temperature, be incubated 1h, guarantee the fabric thorough drying.Speed with 15 ℃/min is warming up to 400 ℃ then, insulation 40min, and the 0.5MPa that pressurizes then removes vacuum, continues insulation 40min, impels carbon fiber bundle impregnated fully.Accelerate speed of cooling when being cooled to 150 ℃ with the rate of temperature fall of 1 ℃/min, the demoulding when products temperature is lower than 100 ℃ can obtain the 3 D weaving carbon fiber reinforced polyether ether ketone matrix material of 18% carbon fiber content, and its microscopic appearance as shown in Figure 1.
Example 2
With carbon fiber volume amount be 36% and PEEK fiber volume amount be 64% blend fiber, ° carry out three-dimensional five by braid angle θ=25 and make the prefabricated component of long 1m, wide 12mm to braiding.Then prefabricated component is put into the (NH that concentration is 3wt%
4)
2HPO
4After boiling 1.5h in the solution, wash repeatedly, be 80 ℃ at oven temperature and carry out drying with deionized water.To cut and be laid in the pre-prepd mould through the three-dimensional shuffling fiber preform of oxide treatment, mould is put into the heating under vacuum jar, and Heating temperature is 170 ℃, and beginning to continue to be evacuated down to vacuum tightness is 70kPa, and under this temperature, be incubated 1h, guarantee the fabric thorough drying.Speed with 15 ℃/min is warming up to 400 ℃ then, insulation 40min, and the 0.8MPa that pressurizes then removes vacuum, continues insulation 40min, impels carbon fiber bundle impregnated fully.Accelerate speed of cooling when being cooled to 150 ℃ with the rate of temperature fall of 1.5 ℃/min, the demoulding when products temperature is lower than 100 ℃ can obtain the 3 D weaving carbon fiber reinforced polyether ether ketone matrix material of 18% carbon fiber content, and its microtexture as shown in Figure 2.
Example 3
With carbon fiber volume amount be 54% and PEEK fiber volume amount be 46% blend fiber, ° carry out three-dimensional five by braid angle θ=25 and make the prefabricated component of long 1m, wide 12mm to braiding.Then prefabricated component is put into the (NH that concentration is 3wt%
4)
2HPO
4After boiling 1.5h in the solution, wash repeatedly, be 80 ℃ at oven temperature and carry out drying with deionized water.To cut and be laid in the pre-prepd mould through the three-dimensional shuffling fiber preform of oxide treatment, mould is put into the heating under vacuum jar, and Heating temperature is 170 ℃, and beginning to continue to be evacuated down to vacuum tightness is 60kPa, and under this temperature, be incubated 1h, guarantee the fabric thorough drying.Speed with 15 ℃/min is warming up to 400 ℃ then, insulation 40min, and the 1MPa that pressurizes then removes vacuum, continues insulation 40min, impels carbon fiber bundle impregnated fully.Accelerate speed of cooling when being cooled to 150 ℃ with the rate of temperature fall of 2 ℃/min, the demoulding when products temperature is lower than 100 ℃ can obtain the 3 D weaving carbon fiber reinforced polyether ether ketone matrix material of 18% carbon fiber content.
Claims (1)
1. the preparation method of a 3 D weaving carbon fiber reinforced polyether ether ketone matrix material is characterized in that may further comprise the steps:
1) polyetheretherketonefiber fiber and carbon fiber are accounted for cumulative volume according to carbon fiber and make prefabricated component to shuffling than for 15-60% carries out three-dimensional five, braid angle θ=25 °, will weave good prefabricated component then is (the NH of 3-10wt% in concentration
4)
2HPO
4Carry out oxide treatment in the solution, take out after boiling 0.5-1.5h, with deionized water rinsing and dry;
2) the three-dimensional shuffling oxidation prefabricated component that step 1) is made is laid in the mould, then mould is put into the heating under vacuum jar, and being 120-170 ℃ in temperature is 10-100kPa with vacuum pressure, and insulation 1-3h obtains the three-dimensional shuffling oxidation of exsiccant prefabricated component;
3) to step 2) to rise to temperature with the temperature rise rate of 10-20 ℃/min be 380-420 ℃ for the exsiccant prefabricated component that obtains, insulation 30-50min, the 0.3-0.8MPa that pressurizes then continues insulation 30-50min;
When 4) sample that step 3) is obtained was cooled to 150-180 ℃ with the rate of temperature fall of 0.5-2 ℃/min, the demoulding obtained 3 D weaving carbon fiber reinforced polyether ether ketone matrix material when continuing cooling again and being lower than 100 ℃.
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| CN 201110020980 CN102167884A (en) | 2011-01-19 | 2011-01-19 | Preparation method of three-dimensional woven carbon fiber reinforced polyetheretherketone composite material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134372A (en) * | 2011-01-20 | 2011-07-27 | 天津市飞荣达科技有限公司 | Three-dimensional braided carbon fiber reinforced polyetheretherketone composite material and preparation method thereof |
| CN103602039A (en) * | 2013-11-13 | 2014-02-26 | 长春工业大学 | Preparation method of carbon fiber reinforced polyether ether ketone composite material |
| CN104005172A (en) * | 2014-05-26 | 2014-08-27 | 东华大学 | Preparation method of blended three-dimensional knitting fabricated part |
| CN104024105A (en) * | 2011-11-30 | 2014-09-03 | 空中客车简易股份公司 | Panel, component for an airplane airfoil comprising the panel, and method for producing the panel |
| CN104497484A (en) * | 2014-12-12 | 2015-04-08 | 天津大学 | Preparation method of three-dimensional woven rubber coating carbon-fiber-reinforced composite material |
| CN105349849A (en) * | 2015-11-24 | 2016-02-24 | 宁波市鄞州永佳连接器件厂（普通合伙） | Telecom connector |
| CN106433036A (en) * | 2016-08-29 | 2017-02-22 | 天津大学 | Method for preparing PVDF modified three-dimensional braided carbon fiber structural damping composite material |
| CN108093320A (en) * | 2017-12-23 | 2018-05-29 | 广州市尊浪电器有限公司 | A kind of Loudspeaker panel |
| CN114561080A (en) * | 2020-11-27 | 2022-05-31 | 天津工业大学 | Electromagnetic shielding material with integrated structure and function and preparation method thereof |
| CN114836899A (en) * | 2022-06-06 | 2022-08-02 | 沈阳富莱碳纤维有限公司 | Method for manufacturing carbon fiber felt |
-
2011
- 2011-01-19 CN CN 201110020980 patent/CN102167884A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库 工程科技I辑》 20090815 李皓 编织纤维增强树脂基复合材料的制备及表面改性研究 B020-11 1 , 第08期 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134372A (en) * | 2011-01-20 | 2011-07-27 | 天津市飞荣达科技有限公司 | Three-dimensional braided carbon fiber reinforced polyetheretherketone composite material and preparation method thereof |
| CN104024105A (en) * | 2011-11-30 | 2014-09-03 | 空中客车简易股份公司 | Panel, component for an airplane airfoil comprising the panel, and method for producing the panel |
| CN103602039A (en) * | 2013-11-13 | 2014-02-26 | 长春工业大学 | Preparation method of carbon fiber reinforced polyether ether ketone composite material |
| CN104005172A (en) * | 2014-05-26 | 2014-08-27 | 东华大学 | Preparation method of blended three-dimensional knitting fabricated part |
| CN104005172B (en) * | 2014-05-26 | 2016-04-06 | 东华大学 | A kind of preparation method of hybrid three-dimensional woven preform |
| CN104497484A (en) * | 2014-12-12 | 2015-04-08 | 天津大学 | Preparation method of three-dimensional woven rubber coating carbon-fiber-reinforced composite material |
| CN105349849A (en) * | 2015-11-24 | 2016-02-24 | 宁波市鄞州永佳连接器件厂（普通合伙） | Telecom connector |
| CN106433036A (en) * | 2016-08-29 | 2017-02-22 | 天津大学 | Method for preparing PVDF modified three-dimensional braided carbon fiber structural damping composite material |
| CN108093320A (en) * | 2017-12-23 | 2018-05-29 | 广州市尊浪电器有限公司 | A kind of Loudspeaker panel |
| CN114561080A (en) * | 2020-11-27 | 2022-05-31 | 天津工业大学 | Electromagnetic shielding material with integrated structure and function and preparation method thereof |
| CN114561080B (en) * | 2020-11-27 | 2024-06-11 | 天津工业大学 | Electromagnetic shielding material with integrated structure and function and preparation method thereof |
| CN114836899A (en) * | 2022-06-06 | 2022-08-02 | 沈阳富莱碳纤维有限公司 | Method for manufacturing carbon fiber felt |
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Application publication date: 20110831 |